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Method for extracting and refining clopyralid

A technology of clopyralid acid and clopyralid acid mother is applied in the field of extraction and purification of clopyralid acid, which can solve the problem of high energy consumption of clopyralid acid technology, and achieve full recovery of effective components, simplification of traditional processes, and high purity. Effect

Active Publication Date: 2013-08-14
ZHEJIANG AVILIVE CHEM CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] Aiming at the defect of high energy consumption in the existing technology of concentrating and extracting clopyralid from clopyralid solution, the present invention provides a method for extracting and refining clopyralid from clopyralid solution prepared by electrochemical reduction

Method used

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  • Method for extracting and refining clopyralid
  • Method for extracting and refining clopyralid

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0034] combine figure 1 and figure 2 , a method for extracting and refining clopyralid:

[0035] By booster pump 2, the mother liquor of clopyralid (content 4.8%) (COD cr=25000mg / L) into the 10μm bag filter 3, and then into the ultrafiltration device 4, the operating pressure is 0.10Mpa, the recovery rate is controlled at 90%, and the ultrafiltration membrane (molecular weight cut-off is 150,000 Daltons) The concentrated liquid I after impurity removal is mixed with the mother liquor of clopyralid for reuse, and the permeate liquid I (turbidity cr =7000mg / L), the permeate III is sent to the secondary product water tank 15; the feed liquid (permeate III) of the secondary product water tank is transported to the three-stage concentration equipment 19 by the high-pressure pump 18, and passes through the three-stage concentration membrane (using Roll-type composite membrane, with a desalination rate of over 95%), the concentrated solution IV obtained after treatment is returned...

Embodiment 2

[0037] combine figure 1 and figure 2 , a method for extracting and refining clopyralid:

[0038] By booster pump 2, the mother liquor of clopyralid (content 3.5%) (COD cr =28000mg / L) into the 10μm bag filter 3, and then into the ultrafiltration device 4, the operating pressure is 0.12Mpa, the recovery rate is controlled at 95%, and the ultrafiltration membrane (molecular weight cut-off is 50,000 Daltons) The concentrated liquid I after impurity removal is mixed with the mother liquor of clopyralid for reuse, and the permeate liquid I (turbidity cr =7500mg / L), the permeate III is sent to the secondary product water tank 15; the feed liquid (permeate III) of the secondary product water tank is transported to the three-stage concentration equipment 19 by the high-pressure pump 18, and passes through the three-stage concentration membrane (using Roll-type composite membrane, with a desalination rate of over 95%), the concentrated liquid IV obtained after treatment is returned t...

Embodiment 3

[0040] combine figure 1 and figure 2 , a method for extracting and refining clopyralid:

[0041] By booster pump 2, the mother liquor of clopyralid (content 5.5%) (COD cr =30000mg / L) into the 10μm bag filter 3, and then into the ultrafiltration device 4, the operating pressure is 0.25Mpa, the recovery rate is controlled at 95%, and the ultrafiltration membrane (molecular weight cut-off is 100,000 Daltons) The concentrated liquid Ⅰ after impurity removal is mixed with the mother liquor of clopyralid for reuse, and the permeate liquid Ⅰ (turbidity cr =7800mg / L), the permeate III is sent to the secondary product water tank 15; the feed liquid (permeate III) of the secondary product water tank is transported to the third-stage concentration equipment 19 by the high-pressure pump 18, and passes through the three-stage concentration membrane (using Roll-type composite membrane, with a desalination rate of over 95%), the concentrated liquid IV obtained by the treatment is returned...

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Abstract

The invention belongs to the field of herbicide preparation, and in particular relates to a method for extracting and refining clopyralid. The method comprises the following steps of: concentrating clopyralid solution prepared by an electrochemical synthesis method by using a membrane concentration and separation technology, pre-treating the concentrate by micro-filtration and ultra-filtration, and purifying the pre-treated concentrate by adopting a multistage membrane concentration process to obtain refined clopyralid. The obtained clopyralid has the characteristics of high purity and good quality, and the high performance liquid chromatography (HPLC) content of the clopyralid reaches over 97 percent; by technical improvement of the traditional process, energy consumption can be reduced,and discharge of waste water and waste gas is reduced; the treated waste water can be directly recycled or discharged after meeting the discharge standard; the method is more favorable for environmental protection; and meanwhile, the yield of the clopyralid is improved.

Description

Technical field [0001] The invention belongs to the field of herbicide preparation, and specifically relates to a method for processing an acid solution, and in particular to a method for extracting and refining clopyralic acid from a clopyralic acid solution prepared by an electrochemical reduction method. Background technique [0002] Clopyralid is a new low-residue herbicide. It is a new nitrogen-containing heterocyclic herbicide with a unique structure, low toxicity, high activity, and environmental friendliness. [0003] At present, there are two main processes for producing clopyridine in China: one is the chemical dechlorination method, which uses excess hydrazine hydrate to reduce tetrachloropicolinic acid in an alkaline aqueous solution to generate clopicolinic acid. This method has low production cost, but has shortcomings such as low product yield and serious environmental pollution. Its maximum yield is 79%, and the product purity is only 90%. Due to the large am...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D213/803
Inventor 李惠跃吴洪星王光辉韦尉玉包进锋陈甘洪云海吕斌
Owner ZHEJIANG AVILIVE CHEM CO LTD
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